技术领域technical field
本发明属于材料科学领域，具体涉及一种铌钛碳复合铝合金变质剂及其制备方法。The invention belongs to the field of material science, and in particular relates to a niobium-titanium-carbon composite aluminum alloy modification agent and a preparation method thereof.
背景技术Background technique
铝合金是应用量最大的金属材料之一，其应用量仅低于钢铁。对金属材料，组织细化是提高材料强度和塑性最有效的方法。与钢铁材料不同，铝合金因没有相变，不能通过热处理的方式细化组织，只能通过变质处理及热变形等手段细化组织。而铸造铝合金，变质处理就成为唯一细化组织、提高铸件性能的关键技术手段，而得到广泛的重视。在变质处理中，变质剂及工艺对组织细化都有显著的影响。目前，在铝合金变质中，应用最多是铝钛硼、铝锶变质剂等。最近、复合稀土、钛的碳化物、钒的碳化物等新的变质剂也开始应用。变质剂细化组织的关键是能够在液相中稳定存在，且界面能够作为异质形核的核心促进形核，细化组织。影响变质效果的另一个因素是变质及铸造工艺。常用的铝钛硼变质剂对冷却速度比较敏感，随冷却速度的降低，其组织明显粗化，导致铸件不同部位因厚度不同而产生明显的组织差异。近来的研究表明，采用铝钛碳变质剂也具有良好的效果。Aluminum alloy is one of the most widely used metal materials, and its application is only lower than that of steel. For metal materials, microstructure refinement is the most effective way to improve the strength and plasticity of materials. Different from steel materials, because aluminum alloy has no phase transition, the microstructure cannot be refined through heat treatment, but can only be refined through metamorphic treatment and thermal deformation. For cast aluminum alloys, modification treatment has become the only key technical means to refine the structure and improve the performance of castings, and has been widely valued. In the modification process, the modification agent and the process have a significant impact on the refinement of the structure. At present, in the modification of aluminum alloys, aluminum titanium boron and aluminum strontium modifiers are most widely used. Recently, new modifiers such as complex rare earths, carbides of titanium, and carbides of vanadium have also begun to be used. The key to refine the structure of the modificator is to be able to exist stably in the liquid phase, and the interface can act as the core of heterogeneous nucleation to promote nucleation and refine the structure. Another factor affecting the effect of deterioration is deterioration and casting process. The commonly used aluminum-titanium-boron modifier is sensitive to the cooling rate. As the cooling rate decreases, its structure will be obviously coarsened, resulting in obvious structural differences in different parts of the casting due to different thicknesses. Recent studies have shown that the use of aluminum titanium carbon modifier also has a good effect.
铝钛碳是利用钛、碳形成碳化钛，钛、铝形成铝三钛，而碳化钛和铝三钛均可以作为铝合金的核心，抑制碳化物的长大，获得更多细小的形核点是有效利用铝钛碳变质效果的关键。铌具有与钛相似的特性，也可以形成碳化铌及铝三铌，且钛和铌和相互替代，形成碳化钛铌和铝三钛铌。另外铌有更大的原子半径，在铝中的扩散更困难，能有效抑制碳化物及铝三钛铌的粗化，从而减少因铸件厚度不同，导致冷却速度不同对变质效果的影响。因此，制备并获得良好变质效果铌钛碳铝合金变质剂将成为细化铝合金铸态组织的关键。AlTiC is the use of titanium and carbon to form titanium carbide, titanium and aluminum to form aluminum tri-titanium, and both titanium carbide and aluminum tri-titanium can be used as the core of aluminum alloys to inhibit the growth of carbides and obtain more fine nucleation points It is the key to effectively utilize the modification effect of aluminum titanium carbon. Niobium has similar characteristics to titanium, and can also form niobium carbide and aluminum niobium, and titanium and niobium can replace each other to form titanium niobium carbide and aluminum niobium trititanium. In addition, niobium has a larger atomic radius and is more difficult to diffuse in aluminum, which can effectively inhibit the coarsening of carbides and aluminum trititanium niobium, thereby reducing the influence of different cooling rates on the metamorphic effect due to different thicknesses of castings. Therefore, preparing and obtaining a good modification effect of niobium titanium carbon aluminum alloy modifier will become the key to refine the as-cast structure of aluminum alloy.
发明内容Contents of the invention
本发明需要解决的技术问题是提供种一种铌钛碳复合铝合金变质剂及其制备方法，使铌、钛、碳具有合理的比例和结构，起到良好的铝合金变质效果，细化铝合金凝固组织。The technical problem to be solved in the present invention is to provide a kind of niobium-titanium-carbon composite aluminum alloy modification agent and its preparation method, so that niobium, titanium and carbon have a reasonable ratio and structure, and have a good effect of modification of aluminum alloy, and refine the aluminum alloy. Alloy solidification structure.
为解决上述技术问题，本发明所采用的技术方案是：一种铌钛碳复合铝合金变质剂，以铌粉、钛粉、石墨粉为原料，所述的铌粉、钛粉的质量比为3:7～7:3；石墨粉与铌粉、钛粉总量的原子比为0.8:1～1:1，上述原料经球磨机械合金化形成铌钛碳复合粉体，其中包含70-80％的碳化钛铌的碳化物颗粒。In order to solve the above-mentioned technical problems, the technical scheme adopted in the present invention is: a kind of niobium-titanium-carbon composite aluminum alloy modification agent, with niobium powder, titanium powder, graphite powder as raw material, the mass ratio of described niobium powder, titanium powder is 3:7～7:3; the atomic ratio of graphite powder to the total amount of niobium powder and titanium powder is 0.8:1～1:1, and the above raw materials are mechanically alloyed by ball milling to form niobium titanium carbon composite powder, which contains 70-80 % titanium carbide niobium carbide particles.
一种铌钛碳复合铝合金变质剂的制备方法，所述方法包括以下步骤：A method for preparing a niobium-titanium-carbon composite aluminum alloy modifier, the method comprising the following steps:
步骤A：以纯度均大于98.0％，其颗粒平均尺寸在300目～1000目之间的铌粉、钛粉、石墨粉为原料；Step A: using niobium powder, titanium powder and graphite powder with a purity greater than 98.0% and an average particle size between 300 mesh and 1000 mesh as raw materials;
步骤B：球磨；Step B: ball milling;
步骤B1：将铌粉、钛粉的质量比为3:7～7:3的混合物料球磨成铌钛合金粉体；Step B1: ball milling the mixture of niobium powder and titanium powder in a mass ratio of 3:7 to 7:3 into niobium-titanium alloy powder;
步骤B2：在步骤B1所得铌钛合金粉体中加入石墨粉，所述石墨粉与铌粉、钛粉总量的原子比为0.8:1～1:1，在氩气的纯度＞99.99％的保护下，进一步球磨使铌钛合金与石墨形成铌钛碳复合粉体，其中包含70-80％的碳化钛铌的碳化物颗粒。Step B2: adding graphite powder to the niobium-titanium alloy powder obtained in step B1, the atomic ratio of the graphite powder to the total amount of niobium powder and titanium powder is 0.8:1 to 1:1, and the purity of the argon gas is >99.99%. Under protection, the niobium-titanium alloy and graphite are further ball-milled to form a niobium-titanium-carbon composite powder, which contains 70-80% of carbide particles of titanium carbide and niobium.
本发明的上述制备方法的进一步改进在于：所述球磨步骤B1是将铌粉与一定比例的钛粉混合后装入球磨罐中，球磨罐中的氧化锆磨球与物料的质量比为15:1～40:1，球磨罐在氩气的纯度＞99.99％的保护下球磨，使铌粉与钛粉形成铌钛合金粉体。The further improvement of the above-mentioned preparation method of the present invention is: the ball milling step B1 is to mix the niobium powder with a certain proportion of titanium powder and then put it into a ball mill jar, and the mass ratio of the zirconia balls in the ball mill jar to the material is 15: 1～40:1, the ball milling tank is ball milled under the protection of argon gas purity >99.99%, so that niobium powder and titanium powder form niobium-titanium alloy powder.
由于采用了上述技术方案，本发明取得的技术进步是：Owing to having adopted above-mentioned technical scheme, the technical progress that the present invention obtains is:
该发明采用机械合金化的方法，使铌钛首先形成合金，然后再与碳形成铌钛碳复合粉体，在复合颗粒中包含了一定量碳化钛铌晶核，且由于机械合金化的作用，铌钛碳复合颗粒中存在大量缺陷及高的机械能，在添加到高温液态铝合金中时，由于高温作用，铌、钛、碳能快速反应，在机械合金化形成碳化物晶核的基础上，生成细小碳化铌钛，并分散到铝合金液中。而少量铌、钛、碳溶入铝合金液在后续的过程中，沿碳化物析出有效促进铝合金凝固组织形核，细化凝固组织。The invention adopts the method of mechanical alloying, so that niobium and titanium form an alloy first, and then form a niobium-titanium-carbon composite powder with carbon. A certain amount of titanium carbide and niobium crystal nuclei are contained in the composite particles, and due to the effect of mechanical alloying, There are a large number of defects and high mechanical energy in niobium-titanium-carbon composite particles. When added to high-temperature liquid aluminum alloy, niobium, titanium, and carbon can react quickly due to high temperature. On the basis of mechanical alloying to form carbide nuclei, Fine niobium titanium carbides are generated and dispersed into the aluminum alloy liquid. A small amount of niobium, titanium, and carbon dissolved in the aluminum alloy liquid will effectively promote the nucleation of the solidification structure of the aluminum alloy along with the precipitation of carbides in the subsequent process, and refine the solidification structure.
本发明的第一次球磨过程实现了铌粉、钛粉的破碎、磨细，同时使铌、钛颗粒内产生大量的空位和位错等缺陷，在铌粉和钛粉的碰撞过程中，不断细化产生大量的新鲜表面以及瞬间的温升促使铌、钛合金化。The first ball milling process of the present invention realizes the crushing and grinding of niobium powder and titanium powder, and at the same time causes defects such as a large amount of vacancies and dislocations to be produced in the niobium and titanium particles. During the collision process of niobium powder and titanium powder, continuous The thinning produces a large number of fresh surfaces and the instantaneous temperature rise promotes the alloying of niobium and titanium.
本发明的第二次球磨过程中，已经机械合金化铌钛合金粉与碳粉在球磨机械能的作用下加速碳的向铌钛合金的扩散，形成铌钛碳复合粉体，并在碰撞温度的作用下，形成碳化物晶核，最终形成包含一定碳化物晶核的铌钛碳复合粉体的铝合金变质剂。In the second ball milling process of the present invention, the mechanically alloyed niobium-titanium alloy powder and carbon powder accelerate the diffusion of carbon to the niobium-titanium alloy under the action of ball milling mechanical energy to form niobium-titanium-carbon composite powder, and at the collision temperature Under the action, carbide crystal nuclei are formed, and finally an aluminum alloy modifier of niobium-titanium-carbon composite powder containing certain carbide crystal nuclei is formed.
具体实施方式detailed description
下面结合实施例对本发明做进一步详细说明：Below in conjunction with embodiment the present invention is described in further detail:
本发明的一种铌钛碳复合铝合金变质剂是以铌粉、钛粉和石墨为原料，所述铌粉、钛粉的质量比为3:7～7:3，石墨粉与铌粉、钛粉总量的原子比为0.8:1～1:1。这种铌钛碳复合铝合金变质由机械合金化方法制备。A kind of niobium-titanium-carbon composite aluminum alloy modifying agent of the present invention is to be raw material with niobium powder, titanium powder and graphite, and the mass ratio of described niobium powder, titanium powder is 3:7～7:3, graphite powder and niobium powder, The atomic ratio of the total amount of titanium powder is 0.8:1-1:1. This niobium-titanium-carbon composite aluminum alloy is modified by a mechanical alloying method.
各实施例所用球磨机均为秦皇岛太极环纳米制品有限公司生产的纳米冲击磨，球磨罐为不锈钢罐，容积为2L，磨球也为氧化锆材质，有φ10mm、磨球的总体积占罐的容积的50％～70％。The ball mill used in each embodiment is a nano-impact mill produced by Qinhuangdao Taijihuan Nano Products Co., Ltd. The ball mill tank is a stainless steel tank with a volume of 2L, and the grinding balls are also made of zirconia. 50% to 70% of that.
实施例1Example 1
第一步：将铌粉(颗粒度为1000目、纯度为99.2％)与钛粉(纯度为98.0％、粒度为1000目)按3:7的质量比混合，装入不锈钢球磨罐中，并按照39:1的球料比(氧化锆磨球与混合粉料的质量比)向磨罐中装入氧化锆球。向球磨罐充入氩气纯度>99.99％，然后在纳米冲击磨上，在300r/min的转速下球磨1小时。Step 1: Mix niobium powder (with a particle size of 1000 mesh and a purity of 99.2%) and titanium powder (with a purity of 98.0% and a particle size of 1000 mesh) in a mass ratio of 3:7, put them into a stainless steel ball mill tank, and Put zirconia balls into the grinding jar according to the ball-to-material ratio (mass ratio of zirconia grinding balls to mixed powder) of 39:1. Fill the ball mill jar with argon gas with a purity >99.99%, and then ball mill it on a nano-impact mill at a speed of 300 r/min for 1 hour.
第二步：在第一步的球磨罐中再加入与铌粉和钛粉原子总和相同的石墨粉(粒度为325目、纯度为99.1％)，充入纯度>99.99％的氩气后，在300r/min的转速下继续球磨3小时。The second step: in the ball mill jar of the first step, add graphite powder (the particle size is 325 orders, the purity is 99.1%) identical with the atomic sum of niobium powder and titanium powder in the ball mill tank of the first step, after filling the argon gas of purity >99.99%, in Continue ball milling for 3 hours at a rotating speed of 300r/min.
所获得的铌钛碳复合铝合金变质剂中铌、钛质量比为3:7。The mass ratio of niobium to titanium in the obtained niobium-titanium-carbon composite aluminum alloy modifier is 3:7.
实施例2Example 2
本实施例与实施例1的区别如下。The difference between this embodiment and Embodiment 1 is as follows.
第一步所用铌粉(颗粒度为1000目、纯度为99.2％)与钛粉(粒度为1000目、纯度为98.0％)按质量比为1:1混合，所使用的氧化锆磨球与铌粉、钛粉混合粉料质量比为30:1，球磨时间1.5小时。The niobium powder used in the first step (the particle size is 1000 mesh, the purity is 99.2%) is mixed with the titanium powder (the particle size is 1000 mesh, the purity is 98.0%) in a mass ratio of 1:1, and the used zirconia grinding balls and niobium The mass ratio of titanium powder and titanium powder mixed powder is 30:1, and the ball milling time is 1.5 hours.
第二步中加入石墨粉(粒度为320目、纯度为99.1％)，石墨粉量与铌粉、钛粉总量的原子比为0.9:1，继续球磨时间为3小时。In the second step, add graphite powder (the particle size is 320 mesh, the purity is 99.1%), the atomic ratio of the amount of graphite powder to the total amount of niobium powder and titanium powder is 0.9:1, and the ball milling time is continued for 3 hours.
所获得的铌钛碳复合铝合金变质剂中铌、钛质量比为1:1。The mass ratio of niobium and titanium in the obtained niobium-titanium-carbon composite aluminum alloy modifier is 1:1.
实施例3Example 3
本实施例与实施例1的区别如下。The difference between this embodiment and Embodiment 1 is as follows.
第一步所用铌粉(颗粒度为1000目、纯度为99.2％)与钛粉(粒度为1000目、纯度为98.0％)按7:3的质量比混合，所使用的氧化锆磨球与铌粉、钛粉混合粉料质量比为30:1，球磨时间1.5小时。The niobium powder used in the first step (the particle size is 1000 mesh, the purity is 99.2%) is mixed with the titanium powder (the particle size is 1000 mesh, the purity is 98.0%) in a mass ratio of 7:3, and the used zirconia grinding ball and niobium The mass ratio of titanium powder and titanium powder mixed powder is 30:1, and the ball milling time is 1.5 hours.
第二步中加入石墨粉(粒度为320目、纯度为99.1％)，石墨粉量与铌粉、钛粉总量的原子比为0.8:1，继续球磨时间为3.5小时。In the second step, add graphite powder (320 meshes, 99.1% purity), the atomic ratio of the graphite powder to the total amount of niobium powder and titanium powder is 0.8:1, and the ball milling time is 3.5 hours.
所获得的铌钛碳复合铝合金变质剂中铌、钛质量比为7:3。The mass ratio of niobium and titanium in the obtained niobium-titanium-carbon composite aluminum alloy modifier is 7:3.
实施例4Example 4
本实施例与实施例1的区别如下。The difference between this embodiment and Embodiment 1 is as follows.
第一步铌粉的粒度为300目，纯度为98.0％，钛粉的粒度为320目，纯度为98.4％的球磨时间为2小时。In the first step, the niobium powder has a particle size of 300 mesh and a purity of 98.0%, and the titanium powder has a particle size of 320 mesh and a purity of 98.4%. The ball milling time is 2 hours.
第二步的球磨时间为4小时。The ball milling time of the second step is 4 hours.
所获得的铌钛碳复合铝合金变质剂中铌、钛质量比为3:7。The mass ratio of niobium to titanium in the obtained niobium-titanium-carbon composite aluminum alloy modifier is 3:7.
实施例5Example 5
本实施例与实施例3的区别如下。The difference between this embodiment and Embodiment 3 is as follows.
第一步铌粉的粒度为300目，纯度为98.0％％，钛粉的粒度为320目，纯度为98.4％的球磨时间为2小时。In the first step, the particle size of the niobium powder is 300 mesh, the purity is 98.0%, the particle size of the titanium powder is 320 mesh, and the purity is 98.4%. The ball milling time is 2 hours.
第二步的球磨时间为4小时。The ball milling time of the second step is 4 hours.
所获得的铌钛碳复合铝合金变质剂中铌、钛质量比7:3。The mass ratio of niobium to titanium in the obtained niobium-titanium-carbon composite aluminum alloy modifier is 7:3.
实施例6Example 6
将所制备的铌钛碳复合铝合金变质剂应用于A356铝合金铸件并与铝钛硼变质剂作对比。具体实施方式如下：The prepared niobium-titanium-carbon composite aluminum alloy modifier was applied to A356 aluminum alloy castings and compared with the aluminum-titanium-boron modifier. The specific implementation is as follows:
将A356铝合金快在中温井式熔化，熔化温度为690℃±5℃。待铝合金完全熔化并达到690℃±5℃后，将与铝合金相比，质量百分数为1.5％的上述实施例1到实施例5所获得的铌钛碳复合铝合金变质剂加入铝液中。加入方法采用铝箔包覆、压入、并搅拌，加入覆盖剂，通氩气出气后浇注。铸模为经300℃预热的热模。为细化A356铝合金中硅相，同时加入质量比为1％的锶变质剂。为和铝钛硼变质剂对比，采用相同工艺制备了铝钛硼变质剂变质的铸锭，铝钛硼变质的加入质量百分比为2％。The A356 aluminum alloy is quickly melted in a well at medium temperature, and the melting temperature is 690°C ± 5°C. After the aluminum alloy is completely melted and reaches 690°C±5°C, the niobium-titanium-carbon composite aluminum alloy modifier obtained in the above-mentioned Examples 1 to 5 with a mass percentage of 1.5% compared with the aluminum alloy is added to the molten aluminum . The addition method is covered with aluminum foil, pressed in, and stirred, and the covering agent is added, and the argon gas is ventilated before pouring. The casting mold is a hot mold preheated at 300°C. In order to refine the silicon phase in the A356 aluminum alloy, a strontium modifier with a mass ratio of 1% was added at the same time. In order to compare with the Al-Ti-B modifier, an ingot modified by the Al-Ti-B modifier was prepared by using the same process, and the addition mass percentage of the Al-Ti-B modifier was 2%.
采用上述实施例1到实施例5所获得的铌钛碳复合铝合金变质剂制备的铸锭材料分别标记为A、B、C、D、E，而采用铝钛硼变质剂制备的铸锭材料标记为F。The ingot materials prepared by using the niobium-titanium-carbon composite aluminum alloy modifiers obtained in the above-mentioned Examples 1 to 5 are respectively marked as A, B, C, D, and E, while the ingot materials prepared by using the aluminum-titanium-boron modifiers are Marked as F.
在铸锭相同的部分切取金相试样及拉伸性能试样，在显微镜下，测量的不同变质剂处理后铸锭A、B、C、D、E、F铝合金枝晶尺寸列于下表；同时，拉伸屈服强度及伸长率也列于下表。Metallographic samples and tensile properties samples were cut from the same part of the ingot, and under a microscope, the dendrite sizes of ingots A, B, C, D, E, and F aluminum alloys after treatment with different modifiers were measured as follows Table; at the same time, the tensile yield strength and elongation are also listed in the table below.
由此可见，在铌钛碳变质剂添加量小于铝钛硼变质剂的条件下，铌钛碳变质剂具有与铝钛硼变质剂相当的变质效果。铌钛碳变质剂在铌钛质量百分比为50:50时，组织细化效果最佳。采用铌钛碳变质剂与铝钛硼变质剂铸锭的性能相比，铌钛碳变质剂使铸件强度略有降低，但是塑性显著增加。It can be seen that under the condition that the amount of the niobium-titanium-carbon modifier is less than that of the aluminum-titanium-boron modifier, the niobium-titanium-carbon modifier has a modification effect equivalent to that of the aluminum-titanium-boron modifier. When the mass percentage of niobium and titanium is 50:50, the structure refinement effect of the niobium titanium carbon modifier is the best. Compared with the properties of ingot casting with niobium-titanium-carbon modifier and aluminum-titanium-boron modifier, the niobium-titanium-carbon modifier slightly reduces the casting strength, but the plasticity increases significantly.
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| CN201610836489.5ACN106244838B (en) | 2016-09-21 | 2016-09-21 | Niobium titanium carbon Al-alloy alterant and preparation method thereof |
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